KR101746039B1 - Method for producing lithium chloride - Google Patents

Method for producing lithium chloride Download PDF

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KR101746039B1
KR101746039B1 KR1020150180909A KR20150180909A KR101746039B1 KR 101746039 B1 KR101746039 B1 KR 101746039B1 KR 1020150180909 A KR1020150180909 A KR 1020150180909A KR 20150180909 A KR20150180909 A KR 20150180909A KR 101746039 B1 KR101746039 B1 KR 101746039B1
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South Korea
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lithium
solution
lithium chloride
separator
membrane
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KR1020150180909A
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Korean (ko)
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박성국
박광석
이상길
이현우
정우철
김기영
위진엽
박운경
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재단법인 포항산업과학연구원
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/04—Halides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/08—Carbonates; Bicarbonates

Abstract

Preparing a raw material solution in which lithium phosphate is dissolved in hydrochloric acid in an equivalent ratio (Li / Cl) of 1.0 to 1.5. And a step of obtaining a lithium chloride aqueous solution from the raw material solution and obtaining an aqueous phosphoric acid solution which is formed as a by-product, using a monovalent ion selective electrodialysis apparatus.

Description

METHOD FOR PRODUCING LITHIUM CHLORIDE [0002]

The present invention relates to a method for producing lithium chloride, and more particularly, to a method for producing lithium chloride using lithium phosphate.

From a commercial standpoint, in order to economically produce lithium hydroxide and lithium carbonate having a purity of a certain concentration or more, it is necessary to remove the impurities present in the lithium-containing solution, but to concentrate the lithium concentration to a proper degree for carbonation.

However, among the total cost, most of the above-mentioned impurity removal cost and lithium concentration cost are problematic, and studies for solving this problem are continuing.

As described above, Patent Documents 1 to 4 are representative examples of commercially available techniques for removing impurities in a lithium-containing solution and concentrating lithium. These commercialized technologies are carried out in the high altitude sea salt lake over 3,000m above sea level and depend on natural evaporation by solar heat. However, such a natural evaporation process generally requires a long period of time of more than one year only for evaporation. In order to shorten the evaporation time, a vast evaporation facility (evaporation use pond) is required. Management and maintenance costs. Moreover, even in the case of the salt water of high precipitation, the natural evaporation process can not be applied even if it is a high quality lithium salt, or the evaporation period is too long, so that a wider evaporation facility is required, and thus economical efficiency can not be secured. In addition, there is a problem in that the chemical cost required for refining specific cations and anions, which are impurities, becomes excessive, and the introduced chemicals become impurities again, which must be purified again.

Various methods have recently been proposed to solve the problems of such commercialized technologies.

Patent Document 5 proposes a lithium concentration method using a vacuum evaporation method in order to avoid excessively wide evaporation facilities and to utilize salt brine in an area with low evaporation amount. However, this technology has the disadvantage that it requires excessive energy cost and economical efficiency.

Patent Document 6 proposes a method of producing lithium carbonate from saline by dissolving lithium phosphate in a chemical method. However, this technique has extremely low solubility of lithium phosphate, which causes various difficult problems to be solved chemically, and since the lithium concentration of the produced lithium phosphate solution is low as it is difficult to dissolve, There is a disadvantage that it necessarily accompanies a high energy enrichment process.

U.S. Patent Publication No. 5219550 US Patent Publication No. 4243392 U.S. Patent No. 4,980,136 German Patent Registration No. 19541558 Korean Patent Registration No. 1238890 Korean Patent Publication No. 10-2010-0077949

One of the objects of the present invention is to provide a process for producing lithium chloride which is excellent in economy and lithium conversion.

According to an aspect of the present invention, there is provided a process for producing a lithium secondary battery comprising the steps of: preparing a raw material solution in which lithium phosphate is dissolved in hydrochloric acid in an equivalent ratio (Li / Cl) of 1.0 to 1.5; Thereby obtaining an aqueous solution of phosphoric acid, which is obtained as a byproduct while obtaining an aqueous solution.

As one of the various effects of the present invention, there is an advantage that the economical efficiency and the lithium conversion ratio are extremely excellent.

The various and advantageous advantages and effects of the present invention are not limited to the above description, and can be more easily understood in the course of describing a specific embodiment of the present invention.

1 is a schematic view schematically showing a monovalent ion-selective electrodialysis apparatus 100. Fig.

Hereinafter, the method for producing lithium chloride of the present invention will be described in detail.

All terms (including technical and scientific terms) used herein can be used in a sense commonly understood by one of ordinary skill in the art to which the present invention belongs, unless otherwise defined. Whenever a component is referred to as "including" an element throughout the specification, it is to be understood that the element may include other elements, not the exclusion of any other element, unless the context clearly dictates otherwise. Also, singular forms may include plural forms unless the context clearly dictates otherwise.

As described above, in order to prepare lithium hydroxide and lithium carbonate from a lithium-containing solution, lithium must be concentrated in the lithium-containing solution. However, all currently used concentration processes require a method of evaporating the water in the solution, so energy is enormously consumed for it, and as a result, the energy enrichment cost is too high to maintain the economical efficiency. It becomes a big obstacle. Therefore, the concentration process is omitted or a minimized economical and efficient method is required, which is the most important factor for the commercialization of the lithium solution.

In order to omit the concentration process, it is necessary to devise a new method for producing a high-concentration lithium chloride aqueous solution or lithium hydroxide aqueous solution which is suitable for the carbonization process of high efficiency. As one of the methods, it is necessary to add phosphoric acid to the lithium- Lithium phosphate which is a stable material is prepared by appropriately adjusting the concentration of lithium phosphate and then lithium phosphate is added to hydrochloric acid which can dissolve easily at a high concentration for effective treatment of lithium phosphate thus obtained to prepare an aqueous lithium chloride solution, A series of process technologies for converting lithium ions into aqueous solutions can be considered.

However, when lithium phosphate is dissolved in hydrochloric acid, a high concentration of lithium chloride aqueous solution can be obtained. However, since this solution contains a large amount of phosphoric acid, lithium carbonate is precipitated together with lithium carbonate when the lithium carbonate is used. In this case, since phosphoric acid used at this time is expensive, it needs to be recycled in the process. If phosphate recovery can not be carried out separately, phosphate cost is added to the manufacturing cost, P), it is a major factor to lower the cost of the process.

Accordingly, the present invention proposes a method of separately separating an aqueous lithium chloride solution and an aqueous phosphoric acid solution from a high concentration aqueous solution of lithium chloride, in which lithium phosphate is dissolved in hydrochloric acid, using a monovalent ion selective electrodialyzer. However, there may be the following additional problems in separating the aqueous solution of lithium chloride and the aqueous solution of phosphoric acid using the monovalent ion-selective electrodialysis device.

High concentration of lithium chloride aqueous solution prepared by dissolving lithium phosphate in hydrochloric acid, the monovalent anions Cl - addition LiHPO4 - and the ion complex is present, such as, 1 a to the H + present in addition to Li + cation due to lithium conversion and current of the lithium chloride In order to maximize the efficiency, it is necessary to understand the electrodialysis behavior of these ions with a kinetics. In addition, when the phosphoric acid component is introduced into the aqueous solution of lithium chloride obtained by electrodialysis, it may cause various problems in the subsequent process of manufacturing the aqueous solution of lithium hydroxide or aqueous solution of lithium carbonate, so that the conversion of lithium to the lithium chloride and the current efficiency It is necessary to devise a method capable of minimizing the inflow of the phosphoric acid component in the aqueous solution of lithium chloride obtained by electrodialysis.

That is, in the present invention, in separating lithium chloride aqueous solution into hydrochloric acid and separately separating the aqueous lithium chloride solution into a lithium chloride aqueous solution and an aqueous phosphoric acid solution by using a monovalent ion selective electrodialysis device, the lithium conversion efficiency and current efficiency into lithium chloride are maximized And a phosphoric acid component in the aqueous lithium chloride solution obtained by electrodialysis can be minimized. Hereinafter, the respective steps will be described in more detail.

Raw material solution preparation process

First, the raw material solution is prepared by dissolving lithium phosphate in hydrochloric acid. As described above, hydrochloric acid can easily dissolve lithium phosphate, which is a stable substance, at a high concentration.

In this step, the equivalence ratio (Li / Cl) of lithium to hydrochloric acid in the raw material solution needs to be appropriately controlled. If the equivalence ratio is too high, the amount of chlorine ions transferred to the lithium ion migration amount in the subsequent electrodialysis process is insufficient, resulting in a reduction in lithium conversion to lithium chloride. On the other hand, if the equivalence ratio is too low, the amount of free hydrogen ions is increased to cause excessive migration of hydrogen ions, and the amount of power required for the movement of each ion is proportional to the equivalent amount of each ion moved according to Faraday's law, As a result, this leads to a decrease in current efficiency.

Taken together, it is necessary to control the equivalence ratio (Li / Cl) of lithium to hydrochloric acid in the raw material solution to 1.0 to 1.5, more preferably 1.07 to 1.25.

Single ion selective electrodialysis process

As described above, in order to recover lithium chloride separately from lithium chloride while obtaining lithium chloride concentrated at a high concentration of lithium, a raw material solution in which lithium phosphate is dissolved in hydrochloric acid is added to a monohydrate-type electrodialysis apparatus together with water To thereby obtain an aqueous solution of lithium chloride and, separately, an aqueous solution of phosphoric acid formed as a by-product.

1 is a schematic view schematically showing a monovalent ion-selective electrodialysis apparatus 100. Fig. 1, a monovalent cation-selective membrane 140 and a monovalent anion-selective membrane 130 that selectively transmit monovalent cation and monovalent anion are provided in the monovalent ion-selective electrodialyzer 100, And may be disposed between the cell and the cathode cell. The anode cell includes a cathode 160 and a cathode separator 150. The cathode cell includes a cathode 110 and a cathode separator 120. The cathode separator includes a cathode 160 and a cathode separator 150, And the negative electrode separator 120. The negative electrode separator 120 may be formed of a non-aqueous electrolyte.

A raw material solution in which lithium phosphate is dissolved in a monovalent acid is applied between the anode separator 150 and the monovalent cation selective membrane 140 of the anode cell and between the anode separator 120 and the monovalent anion- And water can be injected between the monovalent cation-selective membrane 140 and the monovalent anion-selective dialysis membrane 130 to prepare electrodialysis.

A cathode cell and an electrode liquid are each added to the anode cell, for example, lithium sulfate (Li 2 SO 4), lithium hydroxide (LiOH), dihydrogenphosphate lithium (LiH 2 PO 4), phosphoric acid (H 3 PO 4 ), And a combination of these. This electrode solution circulates and smoothes the movement of electrons in each cell.

On the other hand, when an electric current is applied to the monovalent ion-selective electrodialyzer 100 into which the raw material solution and the water are introduced, the anion moves to the anode 160 due to the electrophoresis effect and the cation moves to the cathode 110 do.

Specifically, lithium phosphate and hydrochloric acid in the raw material solution react with each other as shown in the following reaction formula (4). As a result, the ions migrating by the electrophoresis effect are Li + , Cl - , PO 4 3- , H +, and the like.

[Reaction Scheme 4]

Li 3 PO 4 + 3 HCl -> H 3 PO 4 + 3 LiCl

At this time, only Cl - ion, which is a monovalent ion among the anions, can permeate the anion-selective membrane 130 and phosphate ions can not permeate. In addition, the lithium ion, which is a monovalent cation, can transmit the monovalent cation-selective membrane 140 in the direction opposite to the Cl - ion.

Accordingly, Li + ions can be continuously concentrated with the Cl - ion and made into a lithium chloride (LiCl) aqueous solution between the monovalent cation selective membrane 140 and the monovalent anion selective membrane 130. On the other hand, PO from between the anode of the anode cell membrane 150 and the monovalent cation optional permeable membrane 140, and the negative electrode cell cathode separator 120 of the first raw material solution remaining between the anion optional dialysis membrane (130) 43 - Ions and H & lt ; + & gt ; ions are concentrated and made into an aqueous solution of phosphoric acid.

Accordingly, an aqueous solution of lithium chloride (LiCl) is recovered between the monovalent cation-selective membrane 140 and the monovalent anion-selective dialysis membrane 130, and the aqueous solution of phosphoric acid is recovered from the anode separator 150 of the anode cell and the monovalent cation- 140 and between the cathode separator 120 of the cathode cell and the monovalent anion-selective dialysis membrane 130.

As a result, when lithium phosphate dissolved in hydrochloric acid is used as a raw material and a monohydrate-type electrodialysis apparatus 100 is used, an aqueous solution of lithium chloride (LiCl) in which lithium is concentrated at a high concentration is produced, Phosphoric acid (H 3 PO 4 ) aqueous solution.

However, if the conversion rate to the aqueous solution of lithium chloride (LiCl) is excessively increased in this step, the phosphoric acid component is excessively introduced into the aqueous lithium chloride (LiCl) solution, . ≪ / RTI > For example, if the obtained aqueous solution of lithium chloride (LiCl) is to be converted into aqueous lithium hydroxide solution using a bipolar electrodialysis process, it may lead to contamination of the dialysis membrane of the bipolar electrodialysis device.

In addition to Li + , Cl - , PO 4 3 - , and H + dissolved in the hydrochloric acid, LiHPO 4 - , H 2 PO 4 - , Li 2 PO 4 - , LiPO 4 2 - , HPO 4 2 - Ionic complexes are present. Among these ionic complexes, the monovalent ion complexes can migrate with Cl - ions and be included in an aqueous solution of lithium chloride (LiCl). Therefore, it is necessary to find an optimum operating condition that can prevent the excessive permeation of the phosphoric acid component and prevent the contamination of the dialysis membrane in the later process while controlling the conversion rate to the aqueous solution of lithium chloride (LiCl) to an appropriate level. In order to achieve the above object, in the present invention, based on kinetic behavior characteristics in which a chloride ion and a monovalent ion complex move into an aqueous solution of lithium chloride (LiCl) in a raw material solution, the limit of the concentration of phosphoric acid .

Examples of ionic complexes that can be included in the lithium chloride (LiCl) aqueous solution include LiHPO 4 - , H 2 PO 4 - , and Li 2 PO 4 - . These ionic complexes have a large radius and a low migration rate, So that it is difficult to move. On the other hand, chlorine ions are very likely to penetrate the membrane easily. However, when the conductivity of the raw material solution gradually decreases as the movement of chlorine ions progresses, the ion complexes also migrate through the dialysis membrane.

Therefore, it is possible to measure the electric conductivity of the raw material solution, and based on the result, it is possible to achieve the maximization of the conversion ratio to the aqueous solution of lithium chloride (LiCl) and the prevention of the contamination of the dialysis membrane in the post- It is necessary to set the current application end point.

Taking this into consideration, it is preferable to terminate the current application when the phosphorus concentration in the aqueous solution of lithium chloride (LiCl) is 4,000 ppm or less.

On the other hand, the electric conductivity of the raw material solution at the end of current application varies depending on the equivalence ratio (Li / Cl) of lithium to the hydrochloric acid in the raw material solution and their concentration, and is not particularly limited in the present invention.

In this case, as described above, the aqueous phosphoric acid solution is separately recovered. In this case, the separately recovered aqueous phosphoric acid solution can be used as a feed material for the production of lithium phosphate from the lithium-containing solution.

Further, the aqueous solution of lithium chloride (LiCl) separated from the aqueous phosphoric acid solution can be preferably used as a raw material for conversion to aqueous lithium hydroxide solution or lithium carbonate aqueous solution.

Hereinafter, the present invention will be described more specifically by way of examples. It should be noted, however, that the following examples are intended to illustrate and specify the present invention and not to limit the scope of the present invention. And the scope of the present invention is determined by the matters described in the claims and the matters reasonably deduced therefrom.

( Example  One)

Lithium chloride dissolved in hydrochloric acid was used as a raw material, and lithium chloride was prepared using the monovalent ion-selective electrodialyzer shown in Fig. 1. In each example, the electric conductivity of the raw material solution at the end of current application was 30 mS / cm, and the equivalence ratio (Li / Cl) of lithium to hydrochloric acid in the raw material solution was varied. The electrodialysis apparatus used herein was an ASTOM product (effective membrane area: 2 dm 2 , anion / cation dialysis membrane: 60 parts), and the test conditions were set to a temperature of 40 ° C or lower, a voltage of 40 V or lower, and a current of 8 A or lower. The current efficiency and the lithium chloride conversion value in Table 1 below indicate the maximum value and the minimum value of the results measured ten times, respectively.

Equivalent ratio (Li / Cl) One 1.15 1.5 Current efficiency (%) 60 to 68 74 ~ 78 80 ~ 85 Lithium chloride conversion (%) 80 ~ 86 77 ~ 82 68 to 67

Referring to Table 1, the higher the equivalence ratio of lithium to hydrochloric acid in the raw material solution, the higher the current efficiency, but the lower the lithium chloride conversion rate. The lower the equivalence ratio of lithium to hydrochloric acid in the raw material solution, It can be seen that the current efficiency tends to be inversely proportional to the lowering of the current efficiency. When the equivalence ratio falls within the range of 1.07 to 1.25, it can be seen that excellent current efficiency and excellent lithium chloride conversion can be secured at the same time.

( Example  2)

Lithium chloride dissolved in hydrochloric acid was used as a raw material and lithium chloride was prepared using the monovalent ion-selective electrodialysis device shown in Fig. 1. In each example, the equivalent ratio of lithium to hydrochloric acid in the raw material solution (Li / Cl ) Was 1.15, and the electric conductivity of the raw material solution at the end of the current application and the equivalent ratio (Li / Cl) of lithium to hydrochloric acid in the raw material solution were different. The electrodialysis apparatus used herein was an ASTOM product (effective membrane area: 2 dm 2 , anion / cation dialysis membrane: 60 parts), and the test conditions were set to a temperature of 40 ° C or lower, a voltage of 40 V or lower, and a current of 8 A or lower. The conversion of lithium chloride and the concentration of phosphorus in the lithium chloride solution in Table 2 below represent the maximum and minimum values of ten measurements, respectively.

The electric conductivity (mS / cm) of the raw material solution at the end of current application 20 25 30 35 Lithium chloride conversion (%) 88 ~ 93 83 to 89 77 ~ 82 71 ~ 76 In the lithium chloride solution
Phosphorus concentration (ppm) 4,400 to 5,600 3,600 ~ 4,100 1,700 ~ 3,200 800 ~ 1,700

Referring to Table 2, it can be seen that when the electric conductivity of the raw material solution at the end of current application is low, not only the conversion of lithium chloride increases but also phosphorus concentration in the solution tends to increase. As described above, when the conversion of lithium chloride is increased, the consumed amount of the raw material is small, which is advantageous for reducing the manufacturing cost. However, as described above, the increase of the phosphorus concentration in the lithium chloride solution can be prevented by various problems For example, when the obtained aqueous solution of lithium chloride (LiCl) is converted into aqueous solution of lithium hydroxide by using the bipolar electrodialysis process, it may cause a problem of contamination of the dialysis membrane of the bipolar electrodialyser. In order to prevent the problem of contamination of the dialysis membrane of such a bipolar electrodialyser, it is preferable to terminate the application of current at a phosphorus concentration of 4,000 ppm or less. In this embodiment, when the electric conductivity of the raw material solution is 30 mS / cm, It is preferable to terminate the process.

100: 1 ion-selective electrodialysis device
110: cathode
120: cathode separator
130: 1 is anion selective membrane
140: 1 is a cation-selective membrane
150: anode separator
160: anode

Claims (4)

Providing a raw material solution in which lithium phosphate is dissolved in hydrochloric acid in an equivalent ratio (Li / Cl) of 1.0 to 1.5; And
Obtaining a lithium chloride aqueous solution from the raw material solution and obtaining an aqueous phosphoric acid solution which is formed as a byproduct by using a monovalent ion selective electrodialysis device;
≪ / RTI >
The method according to claim 1,
Wherein the raw material solution contains lithium phosphate and hydrochloric acid in an equivalent ratio (Li / Cl) of 1.07 to 1.25.
The method according to claim 1,
The step of obtaining an aqueous solution of phosphoric acid, which is formed as a by-product upon obtaining the lithium chloride aqueous solution,
A cathode cell including a cathode separator, a monovalent anion selective membrane for selectively transmitting a monovalent anion, a monovalent cation selective membrane for selectively permeating a monovalent cation, and a positive electrode comprising a positive electrode separator, Preparing an ion-selective electrodialysis device;
The raw material solution is introduced into the separator membrane of the anode cell and the separator membrane of the separator separately from the separator membrane of the anode cell and between the membrane separator of the cathode cell and the separator membrane of the separator, Into a cation-selective dialysis membrane; And
And a step of applying an electric current to the monovalent ion-selective electrodialyser.
The method according to claim 1,
Wherein the current application is terminated when the concentration of phosphorus in the lithium chloride aqueous solution is 4,000 ppm or less.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109534369A (en) * 2018-12-07 2019-03-29 杭州水处理技术研究开发中心有限公司 A kind of film is integrated to prepare lithium chloride device and method thereof
CN110395749A (en) * 2019-08-09 2019-11-01 山东科技大学 A method of lithium chloride is prepared using the displacement reaction electrodialysis of four compartments

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004142986A (en) * 2002-10-22 2004-05-20 Ind Technol Res Inst Method for manufacturing lithium concentrated liquid from lithium-containing aqueous solution
JP2011168858A (en) * 2010-02-22 2011-09-01 Eco-System Recycling Co Ltd Method for producing high concentration lithium solution from lithium-containing liquid, and method for producing lithium carbonate
KR101193142B1 (en) 2010-08-12 2012-10-22 재단법인 포항산업과학연구원 Manufacturing method of lithium by electrolysis of lithium phosphate aqueous solution

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004142986A (en) * 2002-10-22 2004-05-20 Ind Technol Res Inst Method for manufacturing lithium concentrated liquid from lithium-containing aqueous solution
JP2011168858A (en) * 2010-02-22 2011-09-01 Eco-System Recycling Co Ltd Method for producing high concentration lithium solution from lithium-containing liquid, and method for producing lithium carbonate
KR101193142B1 (en) 2010-08-12 2012-10-22 재단법인 포항산업과학연구원 Manufacturing method of lithium by electrolysis of lithium phosphate aqueous solution

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109534369A (en) * 2018-12-07 2019-03-29 杭州水处理技术研究开发中心有限公司 A kind of film is integrated to prepare lithium chloride device and method thereof
CN109534369B (en) * 2018-12-07 2023-07-28 杭州水处理技术研究开发中心有限公司 Membrane integrated lithium chloride preparation equipment and method thereof
CN110395749A (en) * 2019-08-09 2019-11-01 山东科技大学 A method of lithium chloride is prepared using the displacement reaction electrodialysis of four compartments

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